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Preparation method of ordered mesoporous nano-silica microspheres

A nano-silica and microsphere technology, applied in the field of inorganic mesoporous materials, can solve the problems of long synthesis time and cumbersome operation, and achieve the effects of short reaction time, simple and easy-to-control preparation conditions, and uniform pore size

Active Publication Date: 2018-06-22
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the hydrothermal synthesis method is the main synthesis method for mesoporous silica materials, but the synthesis time is long (at least ten hours) and the operation is cumbersome. Therefore, a new synthesis method that is time-saving, energy-saving and easy to operate is explored. An important problem facing the research of mesoporous nanomaterials

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  • Preparation method of ordered mesoporous nano-silica microspheres
  • Preparation method of ordered mesoporous nano-silica microspheres
  • Preparation method of ordered mesoporous nano-silica microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Dissolve 0.10 g of cetyltrimethylammonium bromide (CTAB) in 60 g of deionized water, add 0.06 g of NaOH, and stir at 80° C. for 120 min at a speed of 200 r / min. Add 0.80 g tetraethyl orthosilicate (TEOS), and continue to stir at 80° C. at a speed of 200 r / min for 8 h. The solution after the reaction is centrifuged (8500r / min), the surfactant template is washed away with deionized water and absolute ethanol, and the ordered mesoporous nano-silica can be obtained after drying in an oven. The mass of the generated product was 0.2115 g, and the yield was 91.7%.

[0027] From figure 1 It can be seen that the ordered mesoporous nano-silica microspheres have a particle diameter of about 150 nm and a pore diameter of about 2.5-3 nm.

Embodiment 2

[0029] Dissolve 0.20 g of cetyltrimethylammonium bromide (CTAB) in 80 g of deionized water, add 0.05 g of NaOH, and stir at 80° C. for 120 min at a speed of 300 r / min. Add 1.00 g of tetraethyl orthosilicate (TEOS), and continue stirring at 80° C. at a speed of 300 r / min for 8 h. The solution after the reaction is centrifuged (8500r / min), the surfactant template is washed away with deionized water and absolute ethanol, and the ordered mesoporous nano-silica can be obtained after drying in an oven. The mass of the generated product was 0.2682 g, and the yield was 93.0%.

[0030] From figure 2 It can be seen that the ordered mesoporous nano-silica microspheres have a particle diameter of about 110 nm and a pore diameter of about 2.5-3 nm.

Embodiment 3

[0032] Dissolve 0.30 g of cetyltrimethylammonium bromide (CTAB) in 70 g of deionized water, add 0.08 g of NaOH, and stir at 70° C. for 90 min at a speed of 500 r / min. Add 1.20 g of tetraethyl orthosilicate (TEOS), and continue stirring at 70° C. at a speed of 500 r / min for 10 h. The solution after the reaction is centrifuged (7500r / min), the surfactant template is washed away with deionized water and absolute ethanol, and the ordered mesoporous nano-silica can be obtained after drying in an oven. The mass of the generated product was 0.3113 g, and the yield was 90.0%.

[0033] From image 3 It can be seen that the ordered mesoporous nano-silica microspheres have a particle diameter of about 130 nm and a pore diameter of about 2.5-3 nm.

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Abstract

The invention discloses a preparation method of ordered mesoporous nano-silica microspheres. A cationic surfactant is dissolved in deionized water; then, inorganic alkaline is added; uniform mixing isperformed under the heating condition; then, a silicon source is added; stirring is performed for 4h to 10h; centrifugation, washing and drying are performed to obtain the ordered mesoporous nano-silica microspheres, wherein the mass ratio of the surfactant to the silicon source is (0.10 to 0.40):(0.60 to 1.50). The ordered mesoporous nano-silica microsphere prepared by the method has small graindiameter, uniform pore diameter, ordered mesoporous channel long range and high yield being 90 percent or higher. The goal of fast producing the nano-silica microspheres with ordered mesoporous channel height in large scale under the condition of low energy consumption can be realized. The preparation method has the advantages that the operation is simple; the reaction time is short; the requiredconditions are mild and can be easily controlled; the synthesis cost is low; the environment-friendly effect is achieved, and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic mesoporous materials, and in particular relates to a preparation method of ordered mesoporous nano silicon dioxide microspheres. Background technique [0002] Ordered mesoporous silica materials have large specific surface and pore volume, adjustable pore size, and long-range uniform ordered pore structure, so they are widely used in the fields of separation, catalysis, adsorption, and biomedicine. In 1992, Mobil successfully synthesized a series of ordered mesoporous silica molecular sieves M41S (MCM-41, MCM-48, MCM-50) using methane quaternary ammonium salt cationic surfactant as a template for the first time. In recent years, in order to realize the wide application of ordered mesoporous silica in different fields, scientific researchers have devoted themselves to optimizing its preparation method, mainly by adjusting the influencing factors of the formation of silica nanoparticles, such as: ...

Claims

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Application Information

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IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/04C01P2004/62C01P2006/16
Inventor 马建中董雨菲刘超鲍艳
Owner SHAANXI UNIV OF SCI & TECH
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